CN105442326B - 一种纳米复合抗紫外有机涂层整理剂及其制备方法 - Google Patents
一种纳米复合抗紫外有机涂层整理剂及其制备方法 Download PDFInfo
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- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
本发明公开了一种纳米复合抗紫外有机涂层整理剂及其制备方法，该有机涂层整理剂由20.0～30.0份聚醚基甲基硅氧烷‑co‑二苯甲酮衍生物基甲基硅氧烷‑co‑二甲基硅氧烷共聚物、5.0～15.0份羟基聚醚封端的聚对苯二酸乙二醇酯、4.5～10.0份水分散型苯基改性硅/钛溶胶、2.0～3.0份水溶性硅烷偶联剂、10.0～20.0份水性聚氨酯粘合剂、0.3～0.5份分散剂、0.5～3.0份增稠剂、0.1～0.5份消泡剂、0.1～0.3份有机锡乳催化剂及12.0～31.0份H2O组成，将本发明制备的纳米复合抗紫外有机涂层整理剂刮涂在涤纶等表面，再经烘干定型，能使布样产生良好的防紫外效果以及滑爽、弹挺手感。
Description
技术领域
本发明属精细化工领域，具体涉及一种具有抗紫外功能的纳米复合有机硅整理剂及其制备方法。
背景技术
紫外(UV)线，亦即波长处于180～400nm的光线，它不仅可引起皮肤表层毛细血管扩张、发红发炎、色素沉积及DNA损伤，而且能诱发皮肤癌。据报道，欧美约1/3左右的皮肤癌患者可能均与接受过量紫外光线照射有关。因此，如何防紫外成为颇受关注的一个课题。
用含有共轭芳基的紫外线吸收剂如2,4-二羟基二苯甲酮衍生物、苯并三氮唑衍生物(CN 103774417、103726313)或UV屏蔽剂(如无机纳米TiO2、ZnO粉体或溶胶，见CN101768854和CN104452295)处理织物，能改善织物的抗紫外功能，并对人体起防护作用。而将UV吸收剂与屏蔽剂相结合，能综合二者的优点，这已成为构筑防紫外涂层最有效的方法之一(CN101768854、103451949、103726313、103774417等)。
但单纯用有机小分子紫外吸收剂和无机纳米屏蔽剂所构建的涂层，手感往往较硬，且柔韧性与附着力较差、易脱落。
发明内容
本发明的目的在于提供一种纳米复合抗紫外有机涂层整理剂及其制备方法，该有机涂层整理剂用于织物的整理，既能赋予织物持久性抗紫外性能，又能赋予织物较柔软的手感。
为达到上述目的，本发明采用了以下技术方案：
一种纳米复合抗紫外有机涂层整理剂，该有机涂层整理剂按质量份数由下列组分组成：20.0～30.0份聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物(UV-1)、5.0～15.0份羟基聚醚封端的聚对苯二酸乙二醇酯(UV-2)、4.5～10.0份水可分散型苯基改性硅/钛溶胶、2.0～3.0份水溶性硅烷偶联剂、10.0～20.0份水性聚氨酯粘合剂、0.3～0.5份分散剂、0.5～3.0份增稠剂、0.1～0.5份消泡剂、0.1～0.3份有机锡乳催化剂以及12.0～31.0份H2O。
所述聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物(UV-1)的结构如式(1)所示：
所述聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物(UV-1)是用Si-H含量为0.16％以及黏度为100～143mPa·s的三甲基硅封端的二甲基硅氧烷-co-氢甲基硅氧烷共聚物(PHMS，咸阳秦阳化工厂)与烯基混合物经硅氢化加成反应而制成，所述烯基混合物由烯丙基聚氧乙烯聚氧丙烯醚(F6)、4-(β-羟基-γ-烯丙氧)丙氧基-2-羟基二苯甲酮(MUV-0)以及乙烯基三乙氧基硅烷(VTES)三种物质组成；所述烯丙基聚氧乙烯聚氧丙烯醚(F6)的结构为CH2＝CHCH2O(C2H4O)a(C3H6O)bH，平均分子量为1300左右；所述三甲基硅封端的二甲基硅氧烷-co-氢甲基硅氧烷共聚物(PHMS)中Si-H键与所述烯基混合物中C＝C双键的摩尔比为1:1.05，烯丙基聚氧乙烯聚氧丙烯醚(F6):4-(β-羟基-γ-烯丙氧)丙氧基-2-羟基二苯甲酮(MUV-0):乙烯基三乙氧基硅烷(VTES)的摩尔比为5:4:1，硅氢化加成反应的温度为80～90℃，反应时间为3～4h；a、b、n、m1、m2及m3为0,1,2,3,…正整数，a:b＝7:3，a+b＝25，m1:m2:m3＝1:5:4，而m1+m2+m3与n的比值取决于原料PHMS中Si-H含量和平均分子量。
所述羟基聚醚封端聚对苯二酸乙二醇酯(UV-2)的结构如式(2)所示，平均分子量为1500～1700：
所述羟基聚醚封端聚对苯二酸乙二醇酯(UV-2)是在对甲苯磺酸作用下用对苯二甲酸(TPA)与乙二醇(EG)以及聚氧乙烯聚氧丙烯醚(PEP)按对苯二甲酸(TPA)：乙二醇(EG)：聚氧乙烯聚氧丙烯醚(PEP)的摩尔比＝(4～3):(3～2):2进行分步酯化反应制备而成，所述聚氧乙烯聚氧丙烯醚(PEP)的结构为HO(C2H4O)a1(C2H4O)b1H、平均分子量为500且a1:b1＝7:3，所述酯化反应温度为80～85℃，总反应时间为10～12h；x取值由TPA与EG的摩尔比所决定、其值为2～3。
所述水可分散型苯基改性硅/钛溶胶选自水可分散型且经苯基改性过的纳米SiO2溶胶、纳米TiO2溶胶或二者任意比例的混合物，含固量为30～35％，粒径为20～30nm，用苯基三乙氧基硅烷与正硅酸乙酯、正钛酸异丙酯或二者任意比例混合物按摩尔比1:5～10在碱性条件下水解缩聚制备或从有关公司购买，如青岛微纳硅胶科技有限公司、山东大易化工有限公司等。
所述水溶性硅烷偶联剂选自2,3-环氧丙氧丙基三甲氧基硅烷(KH-560)或者2,3-环氧丙氧丙基甲基二甲氧基硅烷(KH-561)，或选自平均分子量为300～500的2,3-环氧丙基聚氧乙烯聚氧丙烯丙基三甲氧基硅烷、2,3-环氧丙基聚氧乙烯聚氧丙烯丙基三乙氧基硅烷、聚氧乙烯聚氧丙烯丙基三甲氧基硅烷或聚氧乙烯聚氧丙烯丙基三乙氧基硅烷。
所述水性聚氨酯粘合剂选自端基临时封闭、水溶性而当温度>100℃时可释放出NCO基团的聚醚型聚氨酯或聚酯型聚氨酯，如CX-9038(含固量约为35％，从湖北枣阳创鑫化工公司购买)；所述分散剂为对无机纳米溶胶有良好的润湿分散作用的烷基芳醚或聚丙烯酸铵盐(例如，德国迪高公司生产的Tego 752W)；所述增稠剂为阴离子水溶性聚丙烯酸类增稠剂(例如，北京宝威乳液有限公司、广州市卓能贸易有限公司生产的TA-70)或水溶性非离子缔合型疏水改性的聚氨酯类增稠剂(例如，广州昂迪化工有限公司生产的8W)；所述消泡剂为水性体系使用、且有良好消泡作用的有机硅或脂肪族矿物油类消泡剂(例如Wacker公司的SR-30)；所述有机锡乳催化剂为二月桂酸二正辛基锡、二月桂酸二丁基锡或二醋酸二丁基锡的乳液，含固量为30％。
经所述有机涂层整理剂处理后的织物的阳光防护因子UPF>40，表现出良好的防紫外效果以及滑爽、弹挺手感，所述处理包括以下步骤：将所述有机涂层整理剂用刮刀均匀刮涂在织物表面，然后于100～105℃干燥5～10min，再在150～170℃定型1.5～3min，然后于室温平衡24h。
上述纳米复合抗紫外有机涂层整理剂的制备方法，包括以下步骤：
将计量的H2O、聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物(UV-1)以及羟基聚醚封端的聚对苯二酸乙二醇酯(UV-2)搅拌混匀，得混合物料A，向混合物料A中再加入分散剂、消泡剂以及水可分散型苯基改性硅/钛溶胶后用转速为300～500r/min的磨砂机研磨分散1.5～2h得混合物料B，向混合物料B中再加入水溶性硅烷偶联剂以及水性聚氨酯粘合剂后继续研磨10～30min得混合物料C，向混合物料C中再加入增稠剂以及有机锡乳催化剂后搅拌均匀，得所述有机涂层整理剂，所述有机涂层整理剂的黏度为2500～5000mPa·s。
本发明的有益效果体现在：
本发明将有柔软作用的紫外光吸收剂聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物(UV-1，有效紫外吸收范围λmax＝243～325nm)、无机纳米UV屏蔽剂水可分散型苯基改性硅/钛溶胶与具有UV吸收功能且水可分散的羟基聚醚封端聚对苯二酸乙二醇酯(UV-2)相结合，再配合以水溶性硅烷偶联剂以及水性聚氨酯粘合剂交联固定，利用UV吸收组分与纳米屏蔽剂、粘合剂、偶联剂多组分之间的协同增效与固定作用，不仅能获得所期望的抗紫外效果、解决涂层固定与手感问题，而且能使织物的防紫外效果持久。
具体实施方式
下面结合实施例对本发明做详细说明。
本发明以具有柔软作用的聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物作紫外吸收组分、以苯基改性的纳米硅/钛溶胶作UV屏蔽剂，然后将二者与附着力强的聚氨酯粘合剂以及偶联剂相结合，从而制得了一种可用于织物防紫外整理的纳米复合抗紫外有机涂层整理剂。将其用于织物整理，可获得柔韧与持久抗紫外兼备的效果。具体描述如下：
实施例1
(1)水溶性紫外吸收组分——聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物(UV-1)的合成
在装置有搅拌器、回流冷凝管、温度计的三颈瓶中依次加入10g Si-H含量为0.16％、黏度为100mPa·s的三甲基硅封端的二甲基硅氧烷-co-氢甲基硅氧烷共聚物(PHMS，含Si-H 0.016mol)、10.92g结构为CH2＝CHCH2O(C2H4O)a(C3H6O)bH、平均分子量为1300左右、a:b＝7:3的烯丙基聚氧乙烯聚氧丙烯醚(F6)、2.21g 4-(β-羟基-γ-烯丙氧)丙氧基-2-羟基二苯甲酮(MUV-0)以及0.32g乙烯基三乙氧基硅烷(VTES)，搅拌混匀，加热升温至80℃，再加入50ppm H2PtCl6(催化剂)，然后控温80～90℃连续反应4h。反应结束，得浅棕色透明液体，即水溶性聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物，记作UV-1，黏度约3680mPa·s。
(2)水溶性紫外吸收组分——羟基聚醚封端聚对苯二酸乙二醇酯(UV-2)的合成
在500mL的三颈瓶中依次加入66.4g对苯二甲酸(TPA)、18.62g乙二醇(EG)、199.2g苯、1.3g对甲苯磺酸以及2～3粒沸石，加热升温至80～85℃用油水分离器——索氏提取仪连续提水4h，然后再加入100.0g结构为HO(C2H4O)a1(C2H4O)b1H、平均分子量为500、a1:b1＝7:3的聚氧乙烯聚氧丙烯醚(PEP)，再继续提水6h至出水量达到理论值。然后，在80～85℃先常压蒸馏回收苯溶剂，然后再在P表为500～650mmHg和80～85℃下减压蒸除残留苯并脱低沸15min，反应结束，得黏稠～半流动性液体，即羟基聚醚封端聚对苯二酸乙二醇酯，平均分子量为1700，记作UV-2，参见式(2)，x取值为3。
(3)纳米复合抗紫外有机涂层整理剂的配制
准确称取23.4g H2O、30.0g上述部分(1)制备的UV-1以及15.0g上述部分(2)制备的UV-2，搅拌使物料分散混合均匀，再加入0.4g分散剂(Tego 752W)、0.1g消泡剂(SR-30)以及4.5g水可分散型苯基改性纳米SiO2溶胶(含固量为30％)，用转速为300～500r/min的磨砂机研磨分散2h，然后再加入2.0g水溶性硅烷偶联剂(KH-560)以及10.0g水性聚氨酯粘合剂(CX-9038)，研磨30min使物料混合均匀，再加0.5g增稠剂(8w)以及0.1g有机锡乳催化剂(二月桂酸二丁基锡的乳液，含固量为30％)，搅拌均匀，所得产品即纳米复合抗紫外有机涂层整理剂，记为Anti UV-1，黏度约为2500mPa·s。
实施例2
准确称取18.21g H2O、25.0g实施例1所采用的UV-1以及10.0g实施例1所采用的UV-2，搅拌使物料分散混合均匀，再加入0.4g分散剂(Tego 752W)、0.1g消泡剂(SR-30)以及10.0g水可分散苯基改性纳米TiO2溶胶(含固量为30％)，用转速为300～500r/min的磨砂机研磨分散2h，然后再加入3.0g水溶性硅烷偶联剂(KH-561)、20.0g水性聚氨酯粘合剂(CX-9038)，研磨30min使物料混合均匀，再加入3.0g增稠剂(TA-70)以及0.15g有机锡乳催化剂(二醋酸二丁基锡的乳液，含固量为30％)，搅拌均匀，所得产品即纳米复合抗紫外有机涂层整理剂，记为Anti UV-2，黏度约为4800mPa·s。
实施例3
准确称取21.4g H2O、25.0g实施例1所采用的UV-1以及15.0g实施例1所采用的UV-2，搅拌使物料混合均匀，再加入0.3g分散剂(Tego 752W)、0.3g消泡剂(SR-30)以及10.0g水可分散型苯基改性纳米SiO2/TiO2杂化溶胶(含固量为30％)，用转速为300～500r/min的磨砂机研磨分散2h，然后再加入3.0g水溶性硅烷偶联剂(平均分子量为300的2,3-环氧丙基聚氧乙烯聚氧丙烯丙基三甲氧基硅烷)以及15.0g水性聚氨酯粘合剂(CX-9038)，研磨30min使物料混合均匀，再加1.8g增稠剂(8W)以及0.27g有机锡乳催化剂(二月桂酸二丁基锡的乳液，含固量为30％)，搅拌均匀，所得产品即纳米复合抗紫外有机涂层整理剂，记为Anti UV-3，黏度约为3900mPa·s。
实施例4
准确称取16.2g H2O、20.0g实施例1所采用的UV-1以及12.0g实施例1所采用的UV-2，搅拌使物料混合均匀，再加入0.4g分散剂(Tego 752W)、0.5g消泡剂(SR-30)以及6.0g水可分散型苯基改性纳米SiO2溶胶(含固量为30％)，用转速为300～500r/min的磨砂机研磨分散2h，然后再加入2.5g水溶性硅烷偶联剂(平均分子量为500的2,3-环氧丙基聚氧乙烯聚氧丙烯丙基三甲氧基硅烷)以及15.0g水性聚氨酯粘合剂(CX-9038)，研磨30min使物料混合均匀，再加2.0g增稠剂(8W)以及0.1g有机锡乳催化剂(二月桂酸二正辛基锡的乳液，含固量为30％)，搅拌均匀，所得产品即纳米复合抗紫外有机涂层整理剂，记为Anti UV-4，黏度约为3100mPa·s。
取实施例1-4的纳米复合抗紫外有机涂层整理剂，用刮刀均匀刮涂在涤纶布样[密度(经向×纬向，根/10cm)：473×218]表面，涂层剂用量约为20～30g/m2，然后将布样置于100℃鼓风烘箱中干燥5min，然后再在170℃定型3min，然后将布样在室温平衡24h后，用触摸法评价手感，然后按AATCC183-2000测定抗紫外效果，按AATCC135-2012标准评价耐洗性并测定洗涤5次后织物的防紫外效果，结果见表1。
表1纳米复合抗紫外有机涂层整理剂处理的织物防紫外效果与手感
Claims (8)
1.一种纳米复合抗紫外有机涂层整理剂，其特征在于：该有机涂层整理剂按质量份数由下列组分组成：20.0～30.0份聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物、5.0～15.0份羟基聚醚封端的聚对苯二酸乙二醇酯、4.5～10.0份水可分散型苯基改性硅/钛溶胶、2.0～3.0份水溶性硅烷偶联剂、10.0～20.0份水性聚氨酯粘合剂、0.3～0.5份分散剂、0.5～3.0份增稠剂、0.1～0.5份消泡剂、0.1～0.3份有机锡乳催化剂以及12.0～31.0份H2O。
2.根据权利要求1所述一种纳米复合抗紫外有机涂层整理剂，其特征在于：所述聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物的结构如式(1)所示：
所述聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物是用Si-H含量为0.16％以及黏度为100～143mPa·s的三甲基硅封端的二甲基硅氧烷-co-氢甲基硅氧烷共聚物与烯基混合物经硅氢化加成反应而制成，所述烯基混合物由烯丙基聚氧乙烯聚氧丙烯醚、4-(β-羟基-γ-烯丙氧)丙氧基-2-羟基二苯甲酮以及乙烯基三乙氧基硅烷组成；所述烯丙基聚氧乙烯聚氧丙烯醚的结构为CH2＝CHCH2O(C2H4O)a(C3H6O)bH，其平均分子量为1300，a:b＝7:3；所述三甲基硅封端的二甲基硅氧烷-co-氢甲基硅氧烷共聚物中Si-H键与所述烯基混合物中C＝C双键的摩尔比为1:1.05，烯丙基聚氧乙烯聚氧丙烯醚:4-(β-羟基-γ-烯丙氧)丙氧基-2-羟基二苯甲酮:乙烯基三乙氧基硅烷的摩尔比为5:4:1，硅氢化加成反应的温度为80～90℃，反应时间为3～4h；n、m1、m2及m3为0,1,2,3,…正整数，m1:m2:m3＝1:5:4，m1+m2+m3与n的比值取决于三甲基硅封端的二甲基硅氧烷-co-氢甲基硅氧烷共聚物中Si-H含量和平均分子量。
3.根据权利要求1所述一种纳米复合抗紫外有机涂层整理剂，其特征在于：所述羟基聚醚封端聚对苯二酸乙二醇酯的结构如式(2)所示：
所述羟基聚醚封端聚对苯二酸乙二醇酯是在对甲苯磺酸作用下用对苯二甲酸与乙二醇以及聚氧乙烯聚氧丙烯醚按对苯二甲酸：乙二醇：聚氧乙烯聚氧丙烯醚的摩尔比＝(4～3):(3～2):2进行分步酯化反应制备而成，所述聚氧乙烯聚氧丙烯醚的结构为HO(C2H4O)a1(C2H4O)b1H，所述酯化反应温度为80～85℃，总反应时间为10～12h；a1:b1＝7:3，x取值由对苯二甲酸与乙二醇的摩尔比所决定。
4.根据权利要求1所述一种纳米复合抗紫外有机涂层整理剂，其特征在于：所述水可分散型苯基改性硅/钛溶胶选自水可分散型且经苯基改性过的纳米SiO2溶胶、纳米TiO2溶胶或二者任意比例的混合物，含固量为30～35％。
5.根据权利要求1所述一种纳米复合抗紫外有机涂层整理剂，其特征在于：所述水溶性硅烷偶联剂选自2,3-环氧丙氧丙基三甲氧基硅烷或者2,3-环氧丙氧丙基甲基二甲氧基硅烷，或选自平均分子量为300～500的2,3-环氧丙基聚氧乙烯聚氧丙烯丙基三甲氧基硅烷、2,3-环氧丙基聚氧乙烯聚氧丙烯丙基三乙氧基硅烷、聚氧乙烯聚氧丙烯丙基三甲氧基硅烷或聚氧乙烯聚氧丙烯丙基三乙氧基硅烷。
6.根据权利要求1所述一种纳米复合抗紫外有机涂层整理剂，其特征在于：所述水性聚氨酯粘合剂选自端基封闭、水溶性且当温度>100℃时可释放出NCO基团的聚醚型聚氨酯或聚酯型聚氨酯；所述分散剂为对无机纳米溶胶有润湿分散作用的烷基芳醚或聚丙烯酸铵盐；所述增稠剂为阴离子水溶性聚丙烯酸类增稠剂或水溶性非离子缔合型疏水改性的聚氨酯类增稠剂；所述消泡剂为水性体系使用的有机硅或脂肪族矿物油类消泡剂；所述有机锡乳催化剂为二月桂酸二正辛基锡、二月桂酸二丁基锡或二醋酸二丁基锡的乳液，含固量为30％。
7.根据权利要求1所述的一种纳米复合抗紫外有机涂层整理剂，其特征在于：经所述有机涂层整理剂处理后的织物的阳光防护因子UPF>40，所述处理包括以下步骤：将所述有机涂层整理剂用刮刀均匀刮涂在织物表面，然后于100～105℃干燥5～10min，再在150～170℃定型1.5～3min。
8.一种制备如权利要求1所述纳米复合抗紫外有机涂层整理剂的方法，其特征在于：包括以下步骤：
将H2O、聚醚基甲基硅氧烷-co-二苯甲酮衍生物基甲基硅氧烷-co-二甲基硅氧烷共聚物以及羟基聚醚封端的聚对苯二酸乙二醇酯搅拌混匀，得混合物料A，向混合物料A中再加入分散剂、消泡剂以及水可分散型苯基改性硅/钛溶胶后用磨砂机研磨分散1.5～2h得混合物料B，向混合物料B中再加入水溶性硅烷偶联剂以及水性聚氨酯粘合剂后继续研磨10～30min得混合物料C，向混合物料C中再加入增稠剂以及有机锡乳催化剂后搅拌均匀，得所述有机涂层整理剂。
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